CN110306256B - Preparation method of high-temperature-resistant para-aramid fiber - Google Patents
Preparation method of high-temperature-resistant para-aramid fiber Download PDFInfo
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- CN110306256B CN110306256B CN201910642627.XA CN201910642627A CN110306256B CN 110306256 B CN110306256 B CN 110306256B CN 201910642627 A CN201910642627 A CN 201910642627A CN 110306256 B CN110306256 B CN 110306256B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
- D01F6/905—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides of aromatic polyamides
Abstract
The invention provides a preparation method of high-temperature-resistant para-aramid fiber, and belongs to the technical field of preparation of para-aramid fiber composite materials. The preparation method specifically comprises the following steps: firstly grinding and drying fullerene, then respectively and accurately metering the fullerene and para-aramid resin and mixing, and then mixing the fullerene/para-aramid resin and H obtained in the step2SO4Respectively metering and mixing to prepare spinning slurry; and finally, defoaming and filtering the spinning slurry, spinning by adopting a dry-jet wet spinning method, and obtaining the fullerene modified para-aramid fiber after coagulating bath, water washing, alkali washing, drying and winding. The high temperature resistance of the para-aramid fiber prepared by the preparation method is obviously improved, so that the para-aramid fiber is more widely applied.
Description
Technical Field
The invention belongs to the technical field of preparation of para-aramid fiber composite materials, and particularly relates to a method for modifying para-aramid fibers by fullerene, aiming at improving the high temperature resistance of the para-aramid fibers.
Background
Para-aramid fiber, also called aramid 1414, is an organic fiber with a macromolecular chain composed of aromatic rings and amido bonds, has the properties of high strength, high modulus and low density, the specific strength of the para-aramid fiber is 5-6 times of steel, the modulus of the para-aramid fiber is 2-3 times of that of steel wire or glass fiber, the toughness of the para-aramid fiber is 2 times of that of the steel wire, the density of the para-aramid fiber is only one fifth of that of the steel wire, and meanwhile, the para-aramid fiber is resistant to high temperature, acid and alkali and corrosion of most organic solvents, so that the para-aramid fiber is widely applied to the aspects of aerospace industry, national defense, automobile industry, body armor, communication cables, sports automobiles and the like. In addition, the para-aramid has the characteristics of high temperature resistance, flame retardance and the like, and is mainly used for fire-fighting clothing, aerospace materials, tire framework materials and the like.
Although the para-aramid has good high temperature resistance, has excellent thermal stability within 440 ℃, and is superior to most chemical fiber substances, the para-aramid is rapidly degraded when the temperature exceeds 460 ℃. Therefore, how to improve the high temperature resistance of the aramid fiber, thereby prolonging the service life of the aramid fiber in a high-temperature environment becomes a problem of great concern to material research and users.
However, due to the regular structure and strong chemical inertia of the para-aramid fiber, the improvement of the high temperature resistance of the para-aramid fiber by a chemical method is difficult, and only other methods can be used. The fullerene has excellent thermal stability, and almost no mass loss is caused at the temperature of 600 ℃. The carbon nanotube, graphene and para-aramid composite material of the carbon congener is disclosed and patented, and the fullerene doped para-aramid of the carbon congener is only reported for the first time.
Disclosure of Invention
The invention aims to provide a preparation method of high-temperature-resistant para-aramid fiber, which specifically adopts fullerene, para-aramid resin and sulfuric acid as raw materials to prepare fullerene modified para-aramid fiber.
In order to achieve the purpose, the invention adopts the technical scheme that:
the above objects are achieved by the features of the independent claims. Further implementations are presented in the dependent claims, the description and the drawings.
A preparation method of high-temperature-resistant para-aramid fiber comprises the following steps:
(1) grinding and drying fullerene for later use;
(2) mixing the fullerene, the para-aramid resin and H in the step (1)2SO4Respectively metering and mixing to prepare spinning slurry;
(3) and (3) defoaming and filtering the spinning slurry obtained in the step (2), spinning by adopting a dry-jet wet spinning method, and then obtaining the high-temperature-resistant para-aramid fiber after coagulating bath, water washing, alkali washing, drying, oiling and winding.
The fullerene is C60, C70, C60, or C70, and when C60 and C70 are used in combination, they may be combined at any ratio. Further, the fullerene is C60.
Furthermore, the particle size of the ground fullerene is less than or equal to 0.5 mu m.
Further, the water content of the fullerene after being dried is less than or equal to 1 percent.
Further, the inherent viscosity of the para-aramid resin is 5.2-6.5 dL/g.
Further, said H2SO4The mass concentration of the catalyst is more than or equal to 99.7 percent.
Further, in the step (2), para-aramid resin and H2SO4Para-aramid resin and H2SO4The mass ratio of the mixture is 19.0-19.7% and 80.3-81%, and the dosages of the fullerene are that of the para-aramid resin and the H2SO40 to 5% of the total mass.
Further, in the step (2), when the spinning slurry is prepared, the fullerene and the para-aramid resin are uniformly mixed, and then the mixture is mixed with H2SO4And (4) mixing. On the basis of the technical scheme, the fullerene/para-aramid resin and H2SO4The measurement mode is weightlessness measurement, and the fullerene/para-aramid resin and H are measured2SO4And (4) mixing.
Further, in the step (2), a screw pulper is used for preparing the spinning slurry, and the screw pulper may be one of a single screw pulper and a double screw pulper. On the basis of the technical scheme, the fullerene/para-aramid resin and H2SO4Entering a screw pulping machine at the temperature of minus 5-15 ℃. On the basis of the technical scheme, the temperature of the meshing zone of the screw pulping machine is-5-15 ℃, and the temperature of the pulping zone is 75-95 ℃.
Further, the step (3) is specifically: and (3) defoaming and filtering the spinning slurry obtained in the step (2), extruding the spinning slurry through a spinning nozzle with the aperture of 60-85 microns, the number of holes of 200-666 and the material of tantalum-iron-tantalum, passing through an air layer with the diameter of 5-12 mm, then entering a water coagulation bath with the temperature of 2-4 ℃ and the acid content of 0-8%, drafting by 4-7 times, washing with deionized water under the condition that the spinning speed is 200-270 m/min, washing with alkaline water with the pH value of 9-10, drying at the temperature of 110-150 ℃, finally oiling and winding into a barrel to obtain the high-temperature resistant para-aramid fiber.
The linear density of the high-temperature-resistant para-aramid fiber prepared by the preparation method is 200D-1500D, the strength is more than or equal to 18.0cN/dtex, and the high-temperature resistance is improved by 7-15%.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention does not need to change the existing para-aramid fiber process equipment, utilizes the existing equipment and technology to the maximum extent, and can carry out industrial production.
2. The para-aramid fiber has excellent continuity and stability in the weaving process and is suitable for large-scale production
3. The fiber prepared by the preparation method has no defect on the surface, and the high-temperature resistance is improved by 7-15% on the premise that the strength of the fiber is more than or equal to 18.0 cN/dtex.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a schematic view of a preparation process of a high-temperature-resistant para-aramid fiber provided by an embodiment of the present invention;
fig. 2 is a thermogravimetric spectrum of a para-aramid fiber doped with fullerene and a para-aramid fiber provided by an embodiment of the present invention; in the figure, a is undoped para-aramid fiber; b is the high temperature resistant para-aramid fiber prepared in example 1; c is the high temperature resistant para-aramid fiber prepared in example 2; d is the high temperature resistant para-aramid fiber prepared in example 3; e is the high temperature resistant para-aramid fiber prepared in example 4;
fig. 3 is a graph showing the strength comparison between a para-aramid fiber doped with fullerene and a para-aramid fiber according to an embodiment of the present invention, wherein a is an undoped para-aramid fiber; b is the high temperature resistant para-aramid fiber prepared in example 1; c is the high temperature resistant para-aramid fiber prepared in example 2; d is the high temperature resistant para-aramid fiber prepared in example 3; and E is the high-temperature resistant para-aramid fiber prepared in example 4.
Detailed Description
The technical solutions in the embodiments of the present invention will be described below with reference to the drawings in the embodiments of the present invention.
Example 1
As shown in fig. 1, the preparation method of the high-temperature resistant para-aramid fiber of the embodiment includes the following steps:
(1) grinding the fullerene C60, wherein the particle size after grinding is less than or equal to 0.1 mu m; drying to make its water content less than 1 per mill;
(2) selecting para-aramid resin with the inherent viscosity of 5.5dL/g and H2SO499.98 percent of para-aramid resin and H2SO4The mass ratio is respectively 19.6 percent and 80.4 percent, and the addition amount of the fullerene C60 is that the para-aramid resin and the H are added2 SO 41% of the total mass; at 5 ℃, firstly mixing fullerene C60 with para-aramid resin, and then mixing fullerene C60/para-aramid resin powder with H2SO4Respectively weighing by a weightlessness scale, feeding the obtained product into a double-screw pulping machine, and respectively setting the temperature of an engagement zone and the temperature of a pulping zone of the double-screw pulping machine to be 5 ℃ and 84 ℃ to prepare spinning slurry;
(3) preparing spinning slurry, defoaming and filtering the spinning slurry, spinning by adopting a dry-jet wet spinning method, extruding the spinning slurry through a spinning cap with the pore diameter of 70 mu m, the pore number of 400 and the material of tantalum-iron-tantalum, passing through an air layer of 8mm, then entering a water coagulation bath with the temperature of 2.5 ℃ and the sulfuric acid content of 2 percent, drafting by 5.5 times, under the condition that the spinning speed is 200m/min, washing with high-purity water at 5 ℃, washing with alkaline water with the pH value of 9.3, drying at 120 ℃, finally oiling and winding into a barrel to obtain the fiber with certain physical and mechanical properties, wherein the linear density is 400D, the tensile strength is 18.5cN/dtex, the high-temperature resistance is improved by 7 percent, and the result is shown in figure 2 and figure 3.
Example 2
As shown in fig. 1, the preparation method of the high-temperature resistant para-aramid fiber of the embodiment includes the following steps:
(1) grinding the fullerene C60, wherein the particle size after grinding is less than or equal to 0.1 mu m; drying to make its water content less than 1 per mill;
(2) selecting para-aramid resin with the inherent viscosity of 6.0dL/g and H2SO499.98 percent of para-aramid resin and H2SO4The mass ratio is respectively 19.4 percent and 80.6 percent, and the addition amount of the fullerene C60 is that the para-aramid resin and the H are added2 SO 43% of the total mass; at 5 ℃, firstly mixing fullerene C60 with para-aramid resin, and then mixing fullerene C60/para-aramid resin powder with H2SO4Respectively weighing by a weightlessness scale, feeding the obtained product into a double-screw pulping machine, and respectively setting the temperature of an engagement zone and the temperature of a pulping zone of the double-screw pulping machine to be 5 ℃ and 84 ℃ to prepare spinning slurry;
(3) preparing spinning slurry, defoaming and filtering the spinning slurry, spinning by adopting a dry-jet wet spinning method, extruding the spinning slurry through a spinning nozzle with the aperture of 70 mu m, the number of holes of 400 and the material of tantalum-iron-tantalum, passing through an air layer of 8mm, then entering a water coagulation bath with the temperature of 2.5 ℃ and the sulfuric acid content of 2 percent, drafting by 6 times, under the condition that the spinning speed is 200m/min, washing with high-purity water at 5 ℃, washing with alkaline water with the pH value of 9.3, drying at 120 ℃, finally oiling, and winding into a barrel to obtain the fiber with certain physical and mechanical properties, wherein the linear density is 400D, the tensile strength is 19.0cN/dtex, the high-temperature resistance is improved by 10 percent, and the result is shown in figure 2 and figure 3.
Example 3
As shown in fig. 1, the preparation method of the high-temperature resistant para-aramid fiber of the embodiment includes the following steps:
(1) grinding the fullerene C60, wherein the particle size after grinding is less than or equal to 0.1 mu m; drying to make its water content less than 1 per mill;
(2) selecting para-aramid resin with the inherent viscosity of 6.2dL/g and H2SO499.98 percent of para-aramid resin and H2SO4The mass ratio is respectively 19.3 percent and 80.7 percent, and the addition amount of the fullerene C60 is that the para-aramid resin and the H are added2 SO 44% of the total mass; at 5 ℃, firstly mixing fullerene C60 with para-aramid resin, and then mixing fullerene C60/para-aramid resin powder with H2SO4Respectively measured by a weightless scale, and fed into a double-screw pulping machineSetting the temperature of the meshing area and the temperature of the pulping area of the rod pulping machine to be 5 ℃ and 84 ℃ respectively, and preparing spinning slurry;
(3) preparing spinning slurry, defoaming and filtering the spinning slurry, spinning by a dry-jet wet spinning method, extruding the spinning slurry through a spinning nozzle with the aperture of 70 mu m, the number of holes of 400 and the material of tantalum-iron-tantalum, passing through an air layer of 8mm, entering a water coagulation bath with the temperature of 2.5 ℃ and the sulfuric acid content of 2 percent, drafting by 6 times, washing with high-purity water at 5 ℃, washing with alkaline water with the pH of 9.3, drying at 120 ℃ under the condition that the spinning speed is 200m/min, oiling, and winding into a barrel to obtain the fiber with certain physical and mechanical properties, wherein the linear density is 400D, the tensile strength is 19.2cN/dtex, the high-temperature resistance is improved by 12 percent, and the result is shown in figure 2 and figure 3.
Example 4
As shown in fig. 1, the preparation method of the high-temperature resistant para-aramid fiber of the embodiment includes the following steps:
(1) grinding the fullerene C60, wherein the particle size after grinding is less than or equal to 0.1 mu m; drying to make its water content less than 1 per mill;
(2) selecting para-aramid resin with the inherent viscosity of 6.5dL/g and H2SO499.98 percent of para-aramid resin and H2SO4The mass ratio is respectively 19.2 percent and 80.8 percent, and the addition amount of the fullerene C60 is that the para-aramid resin and H are added2SO45% of the total mass; at 5 ℃, firstly mixing fullerene C60 with para-aramid resin, and then mixing fullerene C60/para-aramid resin powder with H2SO4Respectively weighing by a weightlessness scale, feeding the obtained product into a double-screw pulping machine, and respectively setting the temperature of an engagement zone and the temperature of a pulping zone of the double-screw pulping machine to be 5 ℃ and 84 ℃ to prepare spinning slurry;
(3) preparing spinning slurry, defoaming and filtering the spinning slurry, spinning by adopting a dry-jet wet spinning method, extruding the spinning slurry through a spinning cap with the pore diameter of 70 mu m, the pore number of 400 and the material of tantalum-iron-tantalum, passing through an air layer of 8mm, then entering a water coagulation bath with the temperature of 2.5 ℃ and the sulfuric acid content of 2 percent, drafting by 6.5 times, under the condition that the spinning speed is 200m/min, washing with high-purity water at 5 ℃, washing with alkaline water with the pH value of 9.3, drying at 120 ℃, finally oiling and winding into a barrel to obtain the fiber with certain physical and mechanical properties, wherein the linear density is 400D, the tensile strength is 18.8cN/dtex, the high-temperature resistance is improved by 15 percent, and the result is shown in figure 2 and figure 3.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. The preparation method of the high-temperature-resistant para-aramid fiber is characterized by comprising the following steps of:
(1) grinding and drying fullerene for later use;
(2) mixing the fullerene, the para-aramid resin and H in the step (1)2SO4Respectively metering and mixing to prepare spinning slurry;
(3) defoaming and filtering the spinning slurry obtained in the step (2), then spinning by adopting a dry-jet wet spinning method, and then obtaining the high-temperature resistant para-aramid fiber after coagulating bath, water washing, alkali washing, drying, oiling and winding;
in the step (1), the particle size of the ground fullerene is less than or equal to 0.5 mu m;
in the step (1), the water content of the fullerene after being dried is less than or equal to 1 percent;
in the step (2), the inherent viscosity of the para-aramid resin is 5.2-6.5 dL/g;
in the step (2), the H2SO4The mass concentration of the active carbon is more than or equal to 99.7 percent;
para-aramid resin and H in the step (2)2SO4Para-aramid resin and H2SO4The mass ratio of the mixture is 19.0-19.7% and 80.3-81%, and the dosages of the fullerene are that of the para-aramid resin and the H2SO41% -5% of the total mass;
in the step (2), the fullerene and the para-aramid tree are firstly used for preparing the spinning slurryMixing with fat, and mixing with H2SO4Mixing;
the step (3) is specifically as follows: and (3) defoaming and filtering the spinning slurry obtained in the step (2), extruding the spinning slurry through a spinning nozzle with the aperture of 60-85 microns, the number of holes of 200-666 and the material of tantalum-iron-tantalum, passing through an air layer with the diameter of 5-12 mm, then entering a water coagulation bath with the temperature of 2-4 ℃ and the acid content of 0-8%, drafting by 4-7 times, washing with deionized water under the condition that the spinning speed is 200-270 m/min, washing with alkaline water with the pH value of 9-10, drying at the temperature of 110-150 ℃, finally oiling and winding into a barrel to obtain the high-temperature resistant para-aramid fiber.
2. The method for preparing the high-temperature-resistant para-aramid fiber according to claim 1, wherein the fullerene is C60 or C70 or a combination of C60 and C70, and the C60 and the C70 are combined in any proportion when used in combination.
3. The method for preparing the high-temperature-resistant para-aramid fiber according to claim 1, wherein in the step (2), a screw pulper is used for preparing the spinning slurry, and the screw pulper is one of a single-screw pulper and a double-screw pulper.
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Effective date of registration: 20221223 Address after: 710000 Room 1502-3, 15/F, Block B, Mid west Land Port Financial Town, No. 99, Gangwu Avenue, Xi'an International Port District, Shaanxi Province Patentee after: Shaanxi Shengshi Chenyang Technology Development Co.,Ltd. Address before: 467000 Gaoyang community, Zhanhe District, Pingdingshan City, Henan Province Patentee before: Gao Jinlu |